Ethyl chloroacetate → 1-Piperidineacetic acid, ethyl ester

HRID 64069

反応式

HRID 64069 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[K+].[K+].Cl[CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16]>CN(C=O)C>[N:1]1([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 7751Ethyl chloroacetateHCID 8082PiperidineHCID 11430Potassium Carbonate

生成物 1

HCID 6434661-Piperidineacetic acid, ethyl ester収率 72%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of piperidine (3.4 g, 40.7 mmol, 1.0 eq) in DMF were added K2CO3 (14 g, 101.0 mmol, 2.5 eq.) and ethyl 2-chloroacetate (4.83 ml, 48.9 mmol, 1.2 eq). The mixture was stirred at RT for 16 h. The mixture was quenched and extracted as in Intermediate Example 5(a). The solvent was distilled off to give the product in 72% yield (5 g). LC-MS (ESI): Calculated mass: 171.1; Observed mass 172.3 [M+H]+ (rt: 0.1 min).

後処理

  1. customThe mixture was quenched
  2. extractionextracted as in Intermediate Example 5(a)
  3. distillationThe solvent was distilled off
  4. customto give the product in 72% yield (5 g)
  5. customObserved mass 172.3 [M+H]+ (rt: 0.1 min)

出典と根拠

ORDレコード
ord-4d5b8ba09a57434995d6e8df42992feb
出典データセット
uspto-grants-2016_09
特許番号
US09447091B2

関連ノート

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